4-Hydrazinylpyridine hydrochloride → N-[2-(3-Methoxy-4-benzyloxyphenyl)-ethylidene]-N'-pyridin-4-yl-hydrazine hydrochloride

HRID 612454

반응식

HRID 612454 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]=[CH:16]OC)=[CH:11][C:10]=1[O:19][CH3:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:21].[NH:22]([C:24]1[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=1)[NH2:23]>C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)C>[ClH:21].[CH3:20][O:19][C:10]1[CH:11]=[C:12]([CH2:15][CH:16]=[N:23][NH:22][C:24]2[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=2)[CH:13]=[CH:14][C:9]=1[O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 223202584-Hydrazinylpyridine hydrochlorideHCID 541262471-Benzyloxy-2-methoxy-4-(2-methoxyvinyl)benzene

생성물 1

HCID 70107929N-[2-(3-Methoxy-4-benzyloxyphenyl)-ethylidene]-N'-pyridin-4-yl-hydrazine hydrochloride수율 61%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 702Ethanol용매

실험 절차

To a stirred solution of 1-benzyloxy-2-methoxy-4-(2-methoxyvinyl)benzene (11.0 g), 4-hydrazinopyridine hydrochloride (6.6 g), and ethanol (150 ml) was added p-toluene sulfonic acid (0.39 g). The reaction mixture was stirred under reflux for 2 hrs and concentrated in vacuo. Recrystallization of the residue from methanol/ether gave 9.48 g (61%) of product, mp 154-155° C.

후처리

  1. temperatureunder reflux for 2 hrs
  2. concentrationconcentrated in vacuo
  3. customRecrystallization of the residue from methanol/ether

출처 및 근거

ORD 기록
ord-b384a5500f894d13a7df96d4374ea1cd
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06004977

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